Phosgene → 6-Fluoro-1,3-benzoxazol-2(3H)-one
反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[OH:9].[C:10](=O)([O-])[O-:11].[K+].[K+].C(Cl)(Cl)=O>C(Cl)Cl.C1(C)C=CC=CC=1>[F:8][C:5]1[CH:6]=[CH:7][C:2]2[NH:1][C:10](=[O:11])[O:9][C:3]=2[CH:4]=1参加物
6
実験手順
To 5.0 g (39.3 mmol) 2-amino-5-fluorophenol in 150 ml of CH2Cl2 at 0° C. was added 13.4 (98 mmol) of potassium carbonate and 23 g(47 mmol) of 20 wt % phosgene in toluene. After warming to room temperature, the reaction was stirred an additional hour before quenching onto 200 ml ice/water. The layers were separated and the aqueous phase was extracted with EtOAc (1×100 ml) before the organics were combined and dried over Na2SO4. The solvent was removed in vacuo to give 5.76 g (96% yield) of the desired product as determined by 1H NMR.
後処理
- custombefore quenching onto 200 ml ice/water
- customThe layers were separated
- extractionthe aqueous phase was extracted with EtOAc (1×100 ml) before the
- dry with materialdried over Na2SO4
- customThe solvent was removed in vacuo
出典と根拠
- ORDレコード
- ord-1fe6c1d619b94bfb81bfcff987718a30
- 出典データセット
- uspto-grants-1996_03
- 特許番号
- US05502027
反応ノート
読み込み中…